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Process of producing p-benzene dicarbonic acid bi(diglycol acrylate)

A technology of diethylene glycol phthalate, phthalic anhydride: diethylene glycol, applied in the field of phthalic acid dual production technology, can solve problems such as organic waste water pollution, and achieve the effect of shortening the process

Inactive Publication Date: 2006-08-16
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to provide a PDDA clean production process with high yield, economic and environmental benefits, and fundamentally solve the problem of organic wastewater pollution in the PDDA production process

Method used

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  • Process of producing p-benzene dicarbonic acid bi(diglycol acrylate)
  • Process of producing p-benzene dicarbonic acid bi(diglycol acrylate)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] First put 74g (0.5mol) of phthalic anhydride, 106g (1.0mol) of diethylene glycol, 20g of toluene, 0.5g of antioxidant, and 15g of sodium bisulfate into the three-port reaction with agitator, water separator and condenser In the bottle, heat with an oil bath. Start stirring, the temperature rises to 150°C, and starts reflux dehydration. When 15.5g of water is separated from the water separator, the temperature is lowered to 60°C. Add 130 g of toluene, 1.0 g of antioxidant, 72 g of acrylic acid, 0.5 g of p-hydroxyanisole, 0.5 g of 2,6-tert-butyl-p-cresol, and 5 g of sodium bisulfate, heat up to 108° C., and start reflux dehydration. When 18g of water was separated from the water separator, the material temperature naturally rose to 118°C, the reaction was stopped, the temperature was lowered to 30°C, and the Buchner funnel was used to filter under reduced pressure.

[0025] Add the filtrate back into the reaction flask, remove the toluene under reduced pressure, the vacu...

Embodiment 2

[0027] Take by weighing 370Kg (2.5Kmol) of phthalic anhydride, 530Kg (5Kmol) of diethylene glycol, 125Kg of toluene, 75Kg of sodium bisulfate, and 2.5Kg of antioxidant, and put them into a 2.5m industrial stainless steel reactor. Heating, starting stirring, raising the temperature to 152°C, and starting reflux dehydration. When the amount of water in the water separator reaches 70Kg, stop the steam heating, and cool down to 60°C with the cooling water coil. Then add 360Kg (5Kmol) of acrylic acid, 600Kg of toluene, 0.5Kg of antioxidant, 1Kg of p-hydroxyanisole, 1Kg of 2,6-tert-butyl-p-cresol, add 25Kg of sodium bisulfate, and heat up to 106°C to start reflux dehydration . When the water separator separates 95Kg of water, the material temperature rises to 120°C. Stop heating, and cool to 35°C with cooling water through a coil. The feed liquid is vacuum pumped to the frame plate filter press for filtration. The filter residue is sent to the dissolution tank for recrystallizat...

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Abstract

The invention discloses an environmental protection producing technique of phthalic acid diethylene glycol diacrylate (PDDA), including the concrete steps as follows: (1) synthesizing bis (diethylene glycol acryl) phthalate in ratio of ortho-phthalic acid to diethylene glycol ester to acrylic acid to sodium bisulfate to methylbenzene to inhibitor to antioxidant 1 (mol) to 1.95-2 (mol) to 5-10 (g) to 0.2-0.5 (mol) to 1.5-2 (g) to 0.1-1 (g); (2) synthesizing bis (diethylene glycol acryl) phthalate by bis (diethylene glycol acryl) phthalate, acrylic acid, sodium bisulfate, methylbenzene, inhibitor and antioxidant in ratio of 1 (mol) to 0.95-2 (mol) to 5-10 (g) to 1.5-3 (mol) to 1.5-2 (g) to 0.5-1 (g); (3) adopting normal-pressure or vacuum filtration; (4) desolventizing at vacuum; (5) detecting product indexes. It is a high-yield PDDA clean producing technique with economic and social benefits, radically solving the pollution problem of organic waste water in PDDA producing course.

Description

technical field [0001] The invention relates to a production process of bis(diethylene glycol acrylate) phthalate. Background technique [0002] Bis(diethylene glycol acrylate) phthalate (hereinafter referred to as PDDA) is an acrylate monomer, which is mainly used as a raw material for resin synthesis, coatings and inks. In recent years, with the rise of UV-curable coatings in my country, PDDA has become more and more widely used as a monomer and film-forming substance of UV coatings, and its usage is increasing year by year. However, the existing PDDA production process basically adopts the traditional process of esterification and washing. There are two major defects in this process: one is that water washing produces a large amount of industrial organic wastewater, which pollutes the water environment; the other is that most of the currently used catalysts use sulfuric acid or p-toluenesulfonic acid, which causes corrosion to equipment. Since this type of catalyst must...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/80C07C67/08C07C67/28
Inventor 单文伟曾光明曹宇彭敏汤杨
Owner HUNAN UNIV